CN1186263C - Continuous quasi-gas phase process and apparatus for preparing spherical nanometer Zr(OH)4 particle - Google Patents
Continuous quasi-gas phase process and apparatus for preparing spherical nanometer Zr(OH)4 particle Download PDFInfo
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- CN1186263C CN1186263C CNB021171831A CN02117183A CN1186263C CN 1186263 C CN1186263 C CN 1186263C CN B021171831 A CNB021171831 A CN B021171831A CN 02117183 A CN02117183 A CN 02117183A CN 1186263 C CN1186263 C CN 1186263C
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Abstract
The present invention relates to a method for continuously preparing spherical Zr (OH) 4 nanometer particles by a quasi-gas phase process. The method comprises the following steps: 1) a zirconium salt solution is pressed into a closed atomizer to be atomized; 2) the superfine droplets of the atomized zirconium salt solution and pure ammonia gas are simultaneously led into a reactor to carry out a precipitation reaction, and spherical Zr (OH) 4 nanometer particles are generated; 3) the generated spherical Zr (OH) 4 nanometer particles are led into a particle collector filled with solvents for recovery. The device comprises the atomizer, the reactor and the particle collector, wherein the upper end of the atomizer is communicated with a protective gas bottle through a latex tube, the atomizer is communicated with the reactor through a latex tube and a droplet guiding tube positioned at the top of the reactor, the bottom of the reactor is communicated with the ammonia gas bottle through an upward-bent ammonia gas draft tube positioned at the bottom of the reactor and a latex tube, the upper part of the reactor is communicated with the particle collector through a latex tube, the inner top of the atomizer is provided with a circular sieve plate with thin holes, and the droplet draft tube extends to the middle part of the reactor. The device has the advantages of simple structure, convenient technological operation, and continuous and bulk production.
Description
Invention field
The invention belongs to the synthetic field of powder, particularly a kind of spherical Zr (OH)
4The continuous quasi-gas phase preparation method and the preparation facilities of nanoparticle.
Background technology
Zr (OH)
4Be that the precipitator method prepare ZrO
2Precursor, directly determining product ZrO
2Pattern and size, and spherical Zr (OH)
4The good fluidity of nanoparticle is easily prepared fine and close ceramic body; Can improve simultaneously with ZrO
2Composite ceramics mechanical property for plasticizing substance.ZrO
2Because its excellent mechanical property, the high rigidity under low heat conductance and good heat-shock resistance and the room temperature can be used as ceramic material again, therefore at aspects such as fuel cell, oxygen sensor and oxygen pumps excellent usage is arranged also.So recent two decades comes, the ZrO with various performances
2The pottery and with ZrO
2For the composite ceramics of transformation toughening material is developed rapidly, be one of stupalith research most active fields.By the good ZrO of precipitator method processability
2The prerequisite of powder is to Zr (OH)
4Effective control of presoma performance, so Zr (OH)
4The quality of presoma performance is to the synthetic ZrO of the precipitator method
2Powder characteristic plays crucial effects.Because Zr (OH)
4Poor stability is not so there is relevant Zr (OH) in the document
4Directly technology of preparing is reported.With Zr (OH)
4Prepare relevant technology and all synthesize ZrO mostly with the precipitator method
2Powder technology interrelates.
Existing Zr (OH)
4Technology of preparing mainly contains following two classes:
1) from zircon (ZrSiO
4) extract in the ore deposit, method has: molten alkaline process, potassium silicofluoride fusion method, lime carbonate sintering process etc., and this class methods production cost is lower, but complex process, particle form is wayward, and dimensional homogeneity is poor, degree of purity of production not high (<99.5%).
2) synthetic technology, method has: direct precipitation method, sluggish precipitation, coprecipitation method, reverse micelle method etc., this class methods production cost is moderate, and technology is simpler, and particle form control is general, and dimensional homogeneity is better, degree of purity of production higher (>99.5%).The ubiquitous defective of these methods is: all be liquid phase reaction, thereby be difficult for obtaining spheroidal particle; Batch operation is wasted time and energy; Can not accomplish scale production.
Summary of the invention
The objective of the invention is to overcome the defective that aforesaid method exists, but and provide the spherical Zr (OH) of a kind of serialization, mass-producing
4The continuous quasi-gas phase preparation method of nanoparticle is by to this method synthetic Zr (OH)
4Nanoparticle carries out suitable postorder to be handled, and just can obtain spheric ZrO
2Nano particle;
Another object of the present invention provides a kind of spherical Zr (OH)
4Nanoparticle quasi-gas phase preparation facilities, this apparatus structure is simple, and is easy to use.
Technical scheme of the present invention is as follows:
Spherical Zr provided by the invention (OH)
4The continuous quasi-gas phase preparation method of nanoparticle, its processing step is as follows:
1) be that the zirconium salt solution of 25.0-40.0% is pressed in the airtight atomizing producer with mass concentration, processing atomizes under normal temperature, normal pressure;
2) zirconium salt solution fine mist and the pure ammonia with atomizing imports in the reactor simultaneously, and the generation precipitin reaction of meeting of zirconium salt solution fine mist and pure ammonia just generates spherical Zr (OH)
4Nanoparticle; Described zirconium salt solution fine mist imports with protective gas, and it is 4-7L/min that its protective gas imports flow; It is 3-5L/min that ammonia imports flow;
3) will generate spherical Zr (OH)
4Nanoparticle imports in the particle collector that fills solvent and reclaims;
Described step 3) reclaims the spherical Zr (OH) that is generated
4The solvent that uses during nanoparticle is water or dehydrated alcohol; Described zirconium salt solution is zirconium oxychloride solution, zirconium nitrate solution or zirconium sulfate solution; Described protective gas is nitrogen, argon gas or other protective gas.
Spherical Zr provided by the invention (OH)
4The continuous quasi-gas phase preparation facilities of nanoparticle, it is characterized in that, comprise atomizing producer 2, reactor 8 and particle collector 7, atomizing producer 2 upper ends are connected with protective gas bottle 1 by emulsion tube 11, be connected with reactor 8 by emulsion tube 21 and the droplet thrust-augmenting nozzle 5 that is positioned at reactor head, reactor 8 bottoms are connected with ammonia bottle 6 by being positioned at its bottom ammonia thrust-augmenting nozzle 4 and emulsion tube 81 of being bent upwards, and reactor 8 wall tops are connected with particle collector 7 by emulsion tube 71; Described atomizing producer 2 inner tops are provided with circular pore sieve plate; Described droplet thrust-augmenting nozzle extends the reactor middle part; Described protective gas bottle 1 is nitrogengas cylinder, argon bottle or other protective gas bottle.
Spherical Zr of the present invention (OH)
4The continuous quasi-gas phase preparation method device of nanoparticle has following characteristics:
1) the employed raw material of the inventive method is cheap, and technology is simple, processing ease, and production cost is low, saves time, and the efficient height can be realized mass-producing, serialization production;
2) device construction of the present invention is simple, and the material range of choice is wide, easily processing.
Description of drawings
Accompanying drawing 1 is the structural representation of device of the present invention:
Accompanying drawing 2-(a) and the spherical Zr (OH) that (b) prepares for inventive method
4The transmission electron microscope pattern picture of nanoparticle;
Wherein: 2 atomizings of nitrogengas cylinder 1 atomizing producer take place 3
Ammonia thrust-augmenting nozzle 4 droplet ingress pipes 5 ammonia bottles 6
Embodiment
Accompanying drawing 1 is the structural representation of apparatus of the present invention, as shown in Figure 1, and spherical Zr of the present invention (OH)
4The continuous quasi-gas phase preparation facilities of nanoparticle, comprise atomizing producer 2, reactor 8 and particle collector 7, atomizing producer 2 upper ends are connected with protective gas bottle 1 by emulsion tube 11, be connected with reactor 8 by emulsion tube 21 and the droplet thrust-augmenting nozzle 5 that is positioned at reactor head, reactor 8 bottoms are connected with ammonia bottle 6 by being positioned at its bottom ammonia thrust-augmenting nozzle 4 and emulsion tube 81 of being bent upwards, and reactor 8 wall tops are connected with particle collector 7 by emulsion tube 71; Described atomizing producer 2 inner tops are provided with circular pore sieve plate; Described droplet thrust-augmenting nozzle extends the reactor middle part; Described protective gas bottle 1 is nitrogengas cylinder, argon bottle or other protective gas bottle.
During use, operation steps is as follows:
1) zirconium salt solution with mass concentration 25.0-40.0% is pressed in the airtight atomizing producer 2, opens 2 atomizings of atomizing producer and takes place 3 zirconium salt solution atomized under normal temperature, normal pressure;
2) open protective gas bottle 1, the zirconium salt solution fine fog is blown in the reactor 8 by importing Glass tubing, protective gas bottle 1 is nitrogengas cylinder, argon bottle or other security protective gas bottle, and its protective gas flow is 4-7L/min;
3) the gaseous tension overgauge normal atmosphere in the reactor 8, the spherical Zr (OH) that generates in the reactor 8
4Nanoparticle is transported in the collector 7 that solvent is housed; The solvent that collector 7 is equipped with is water or dehydrated alcohol.
Embodiment 1:
1) zirconium oxychloride solution with mass concentration 25% is pressed in the airtight atomizing producer 2, and the atomizing of opening atomizing producer 2 takes place 3 zirconium oxychloride solution atomized;
2) open protective gas bottle (nitrogengas cylinder) 1, its nitrogen flow is 4L/min; The zirconium oxychloride aqueous solution fine fog is blown in the reactor 8 by importing Glass tubing;
3) the gaseous tension overgauge normal atmosphere in the reactor 8, the spherical Zr (OH) that generates in the reactor 8
4Nanoparticle is transported in the collector 7 that solvent is housed, and in the collector 7 aqueous solvent is housed.
Embodiment 2:
1) zirconium nitrate solution with mass concentration 30% is pressed in the airtight atomizing producer 2, and the atomizing of opening atomizing producer 2 takes place 3 zirconium nitrate solution atomized;
2) open protective gas bottle (nitrogengas cylinder) 1, its nitrogen flow is 6L/min; The zirconium nitrate solution fine fog is blown in the reactor 8 by importing Glass tubing;
3) the gaseous tension overgauge normal atmosphere in the reactor 8, the spherical Zr (OH) that generates in the reactor 8
4Nanoparticle is transported in the collector 7 that solvent is housed, and collector 7 is equipped with etoh solvent.
Embodiment 3:
1) the zirconium sulfate solution with mass concentration 40% is pressed in the airtight atomizing producer 2, and the atomizing of opening atomizing producer 2 takes place 3 zirconium sulfate solution atomized;
2) open protective gas bottle (argon bottle) 1, its argon flow amount is 7L/min; Zirconium sulfate solution fine fog is blown in the reactor 8 by importing Glass tubing;
3) the gaseous tension overgauge normal atmosphere in the reactor 8, the spherical Zr (OH) that generates in the reactor 8
4Nanoparticle is transported in the collector 7 that solvent is housed; Collector 7 is equipped with etoh solvent.
Claims (5)
1. a spherical Zr (OH)
4The continuous quasi-gas phase preparation method of nanoparticle, its processing step is as follows:
1) be that the zirconium salt solution of 25.0-40.0% is pressed in the airtight atomizing producer with mass concentration, processing atomizes under normal temperature, normal pressure;
2) zirconium salt solution fine mist and the pure ammonia with atomizing imports in the reactor simultaneously, and the generation precipitin reaction of meeting of zirconium salt solution fine mist and pure ammonia just generates spherical Zr (OH)
4Nanoparticle; Described zirconium salt solution fine mist imports with protective gas, and it is 4-7L/min that its protective gas imports flow; It is 3-5L/min that ammonia imports flow.
3) will generate spherical Zr (OH)
4Nanoparticle imports in the particle collector that fills solvent and reclaims; 2. by the described spherical Zr of claim 1 (OH)
4The continuous quasi-gas phase preparation method of nanoparticle is characterized in that, described step 3) reclaims the spherical Zr (OH) that is generated
4The solvent that uses during nanoparticle is water or dehydrated alcohol.
3. by the described spherical Zr of claim 1 (OH)
4The continuous quasi-gas phase preparation method of nanoparticle is characterized in that, described zirconium salt solution is zirconium oxychloride solution, zirconium nitrate solution or zirconium sulfate solution.
4. by the described spherical Zr of claim 1 (OH)
4The continuous quasi-gas phase preparation method of nanoparticle is characterized in that, described protective gas is nitrogen or argon gas.
5. a spherical Zr (OH)
4The continuous quasi-gas phase preparation facilities of nanoparticle, it is characterized in that, comprise atomizing producer (2), reactor (8) and particle collector (7), atomizing producer (2) upper end is connected with protective gas bottle (1) by emulsion tube (11), be connected with reactor (8) by emulsion tube (21) and the droplet thrust-augmenting nozzle (5) that is positioned at reactor head, reactor (8) bottom is connected with ammonia bottle (6) by ammonia thrust-augmenting nozzle (4) and the emulsion tube (81) that is positioned at its bottom and is bent upwards, and reactor (8) wall top is connected with particle collector (7) by emulsion tube (71); Described atomizing producer (2) inner top is provided with circular pore sieve plate; Described droplet thrust-augmenting nozzle extends the reactor middle part.
6. by the described spherical Zr of claim 5 (OH)
4The continuous quasi-gas phase preparation facilities of nanoparticle is characterized in that, described protective gas bottle (1) is nitrogengas cylinder or argon bottle.
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CNB021171831A CN1186263C (en) | 2002-04-25 | 2002-04-25 | Continuous quasi-gas phase process and apparatus for preparing spherical nanometer Zr(OH)4 particle |
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CNB021171831A CN1186263C (en) | 2002-04-25 | 2002-04-25 | Continuous quasi-gas phase process and apparatus for preparing spherical nanometer Zr(OH)4 particle |
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CN1186263C true CN1186263C (en) | 2005-01-26 |
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Families Citing this family (5)
Publication number | Priority date | Publication date | Assignee | Title |
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CN100522822C (en) * | 2006-05-12 | 2009-08-05 | 中国科学院过程工程研究所 | In-situfiguration preparing method for zirconium oxide particle film |
CN103936067B (en) * | 2014-04-03 | 2015-10-28 | 北京工业大学 | A kind of even centrifugal shearing equipment preparing superfine spherical zirconium hydroxide powder |
CN110156070B (en) * | 2019-06-04 | 2021-07-30 | 先导薄膜材料有限公司 | Preparation method of nanoscale indium hydroxide |
CN113277534A (en) * | 2021-05-07 | 2021-08-20 | 李治涛 | Synthesis method of nano-scale magnesium hydroxide |
CN113842854A (en) * | 2021-08-24 | 2021-12-28 | 深圳市银宝山新科技股份有限公司 | Reaction device |
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